Process for producing glycolic acid from formaldehyde and hydrogen cyanide
A technology of glycolic acid and hydrogen cyanide, applied in chemical instruments and methods, cyanide reaction preparation, organic compound preparation, etc., can solve the problem of no nitrilase activity, etc.
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Embodiment 1
[0342] Preheat 90% formaldehyde continuous feed
[0343] About 10.18 g of 52 wt% aqueous formaldehyde (<1% methanol, DuPont) was mixed with 12.81 g of water and the raw meal was heated to about 76°C for about 40 min until the mixture became a clear homogeneous liquid solution. The solution was cooled to room temperature, still a homogeneous liquid. Then, 0.16 mL of 16.7 wt% NaOH aqueous solution was added to the formaldehyde solution. 1.56 g of the as-synthesized solution (23 wt% formaldehyde) was placed in the autoclave and the remainder was used for continuous formaldehyde feed.
[0344] The reaction vessel equipped with stirring was placed in an oil bath maintained at 55°C. An approximately 12-inch section formaldehyde feed line (1 / 16" OD (approximately 1.6 mm) x 0.040" ID (approximately 1.02 mm)) placed directly before the reaction flask inlet was heated to 120°C, then heated for approximately 2.0 hours. The following reactants are each continuously pumped into the re...
Embodiment 2
[0350] Preheating 100% formaldehyde continuous feed
[0351] About 10.18 g of 52 wt% aqueous formaldehyde (<1% methanol, E.I. DuPont de Nemours) was mixed with 12.81 g of water and the raw meal was heated to about 76°C for about 40 min until the mixture became a clear homogeneous liquid solution. The solution was cooled to room temperature, still a homogeneous liquid. Then, 0.14 mL of 16.7 wt% NaOH aqueous solution was added to the formaldehyde solution. The resulting solution (23 wt% formaldehyde) was used for continuous formaldehyde feed.
[0352] A reaction vessel equipped with stirring was charged with a mixture of 0.18 g HCN in 3.4 g water and then placed in an oil bath maintained at 55°C. An approximately 12-inch section formaldehyde feed line (1 / 16" OD x 0.040" ID) placed directly before the reaction flask inlet was heated to 120°C, and the following reactants were each continuously pumped over a period of approximately 2.0 hours Into the reactor:
[0353] 4.41 mL...
Embodiment 3
[0358] Preheating 100% formaldehyde continuous feed
[0359] Approximately 14.20 g of 37 wt% formaldehyde in water (10-15% methanol, Acros Organics, Morris Plains, NJ) was mixed with 8.78 g of water and 0.14 mL of 16.7 wt% NaOH solution. The resulting solution (23 wt% formaldehyde) was used for continuous formaldehyde feed.
[0360] A reaction vessel equipped with stirring was charged with a mixture of 0.18 g HCN in 3.4 g water and then placed in an oil bath maintained at 55°C. An approximately 12-inch section formaldehyde feed line (1 / 16" OD x 0.040" ID) placed directly before the reaction flask inlet was heated to 120°C, and the following reactants were each continuously pumped over a period of approximately 2.0 hours Into the reactor:
[0361] 4.21 mL / hr of 50 wt% HCN in water (d=0.86 g / mL)
[0362] 7.67 mL / hr of 23 wt% aqueous formaldehyde, as described above (d = 1.07 g / mL).
[0363] After about 2.0 hours, the feeds were stopped, the autoclave was removed from the o...
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